Water → HCID 69583568、化合物
反応式
[I-].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2([CH2:12][N+:13]3([CH2:18][CH3:19])[CH2:17][CH2:16][CH2:15][CH2:14]3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.[OH2:20]>>[OH-:20].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2([CH2:12][N+:13]3([CH2:18][CH3:19])[CH2:17][CH2:16][CH2:15][CH2:14]3)[CH2:10][CH2:11]2)=[CH:5][CH:4]=1参加物
実験手順
The hydroxide form of 1-[1-(4-chloro-phenyl)-cyclopropyhnethyl]-1-ethyl-pyrrolidinium cation is obtained by an ion exchange treatment of the iodide salt with Ion-Exchange Resin-OH (BIO RAD® AH1-X8). In a 1-liter volume plastic bottle, 100 gm (255 mmol) of 1-[1-(4-chloro-phenyl)-cyclopropylmethyl]-1-ethyl-pyrrolidinium iodide is dissolved in 300 ml de-ionized water. Then, 320 gm of the ion exchange resin is added and the solution is allowed to gently stir overnight. The mixture is then filtered, and the resin cake is rinsed with minimal amount of de-ionized water. The filtrate is analyzed for hydroxide concentration by titration analysis on a small sample of the solution with 0.1N HCl. The reaction yields 96% of (245 mmol) of the desired 1-[1-(4-chloro-phenyl)-cyclopropylmethyl]-1-ethyl-pyrrolidinium hydroxide (hydroxide concentration of 0.6 M).
後処理
- filtrationThe mixture is then filtered
- washthe resin cake is rinsed with minimal amount of de-ionized water
- concentrationThe filtrate is analyzed for hydroxide concentration by titration analysis on a small sample of the solution with 0.1N HCl
出典と根拠
- ORDレコード
- ord-3bcb5549129f4f7781a17099a365cfae
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07083714B2
反応ノート
読み込み中…